反応 #3098
ord-9216403abe2a471cb8b491c2ec69c28c
反応方程式
反応条件
後処理
- 1温度while warming to ambient temperature
- 2温度The mixture was cooled to 0° C.
- 3workup.STIRRINGThe reaction mixture was stirred 18 hours
- 4温度while warming to ambient temperature
- 5洗浄The reaction mixture was washed with 1M aqueous sodium carbonate solution (30 mL)
- 6乾燥dried over anhydrous sodium sulfate
- 7ろ過filtered
- 8濃縮concentrated under reduced pressure
- 9workup.DISSOLUTIONThe residue was dissolved in ether (2mL)
- 10温度cooled to 0° C. under a nitrogen atmosphere
- 11workup.STIRRINGThe reaction was stirred 18 hours
- 12温度while warming to ambient temperature
- 13濃縮The reaction mixture was concentrated under reduced pressure
- 14その他the residual oil was used in the next step without further purification
実験手順
To 2-propylpentanoic acid (156.6 μl, 1.00 mmol) dissolved in anhydrous dichloromethane (2 mL) was added DMF (3 μL, 4 mole %), and the solution was cooled to 0° C. under a nitrogen atmosphere. To the solution was added oxalyl chloride (94.3 μL, 1.08 mmol) dropwise over a few minutes. The reaction was stirred 18 hours while warming to ambient temperature. The mixture was cooled to 0° C. and excess ~0.3M ethereal diazomethane solution was added. The reaction mixture was stirred 18 hours while warming to ambient temperature. The reaction mixture was washed with 1M aqueous sodium carbonate solution (30 mL), dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure. The residue was dissolved in ether (2mL) and cooled to 0° C. under a nitrogen atmosphere. Hydrogen chloride as a 4N solution in dioxane (275 μL, 1.10 mmol) was added dropwise over a few minutes. The reaction was stirred 18 hours while warming to ambient temperature. The reaction mixture was concentrated under reduced pressure and the residual oil was used in the next step without further purification.